US6387704B1 - Method for compensating for the time-dependent change in coolant level during gas sorption analysis - Google Patents
Method for compensating for the time-dependent change in coolant level during gas sorption analysis Download PDFInfo
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- US6387704B1 US6387704B1 US09/550,887 US55088700A US6387704B1 US 6387704 B1 US6387704 B1 US 6387704B1 US 55088700 A US55088700 A US 55088700A US 6387704 B1 US6387704 B1 US 6387704B1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
- G01N15/0893—Investigating volume, surface area, size or distribution of pores; Porosimetry by measuring weight or volume of sorbed fluid, e.g. B.E.T. method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/0866—Sorption
- G01N2015/0873—Dynamic sorption, e.g. with flow control means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/11—Automated chemical analysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/11—Automated chemical analysis
- Y10T436/115831—Condition or time responsive
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/12—Condition responsive control
Definitions
- This invention concerns sorption analysis and, more specifically, a method for compensating for the time-dependent change in the coolant level surrounding the sample cell during gas sorption analysis.
- the measurement of the amount of gas adsorbed and desorbed by a solid as a function of gas pressure is employed in the determination of surface area, pore size, pore volume and pore area distribution of many solid substances.
- These substances can be non-porous or porous to a greater or lesser extent and can be in the form of monoliths, granules, pellets, tablets, extrudates, powders or other solid form.
- the surface area of a solid is an important physical characteristic which plays a significant role in the behavior of the solid in terms of its interaction with other solid surfaces, liquids, vapors and gases. Pore size, volume and area distributions are important in catalyst selectivity, molecular sieving action, gas and liquid absorption capacity, optical properties of transparent materials and bio-compatibility of implanted materials.
- the method most commonly employed to make these surface area and other determinations is the so-called static volumetric method and requires that the amount of gas adsorbed be measured as a function of applied gas pressure.
- the sample is contained in a sample cell normally constructed of borosilicate glass. Suitable pretreatment of the sample removes unwanted surface contaminants.
- the sample cell containing the sample then is attached to the measuring apparatus and evacuated to remove much of the residual atmosphere or other gas.
- a valve separates the test station, to which the sample cell is attached, from the remainder of the system.
- the void volume is that volume contained within the sample cell and the test station up to that valve and must be known in order to calculate the amount of gas in that void volume. This void volume determination can be achieved in one of at least two ways.
- the void volume is measured immediately prior to the sorption analysis.
- a non-adsorbing gas such as helium, is expanded or dosed from a known, calibrated volume, the dosing manifold, into the sample cell containing the sample.
- the principles of the gas laws primarily Boyle's Law, are applied. This determination must be done both at ambient temperature and then with that portion of the cell containing the sample at the analysis temperature.
- the void volume is not calculated directly, but the amount of analysis gas, the adsorptive that is transferred from the manifold to an empty cell, is measured as a function of pressure, under the same conditions of temperature as the subsequent analysis, and can be done at one or more discrete pressures.
- the analysis temperature normally is no higher than the boiling point of the adsorptive gas. Since the analysis gases most commonly employed are inert, “permanent” gases, the analysis temperature should be that of the liquefied gas. This enhances the adsorption process; therefore, a cryogenic liquid is employed. For example, when nitrogen is used as the adsorptive, the cryogenic liquid most commonly is liquid nitrogen and is held in a Dewar flask into which the sample cell is immersed. After the void volume has been determined in the manner described above, the proportion which is effectively at ambient temperature, the so-called “warm zone”, and that which is effectively at the cryogenic temperature, the so-called “cold-zone”, must remain constant. Only then can the amount of gas in the total void volume be accurately accounted for.
- pressure in the sample cell must increase solely due to the addition of gas from the dosing manifold and not due to the warming of any portion of the void volume.
- the coolant evaporates from the Dewar.
- the cold zone decreases in volume, while the warm zone increases. If this change of coolant level is not compensated for by some means, the measurement of the amount of gas adsorbed is in error, which is a function of both pressure and time.
- Control or maintenance of cryogenic liquid level, the coolant, which surrounds the sample cell, which is changing because of its continuing evaporation, can be achieved in a number of ways:
- the coolant can be replenished during the analysis by transferring coolant from a storage vessel to the Dewar, in response to the output of an electronic circuit monitoring coolant level, as employed in Micromeritics® Digisorb 2600, Coulter® Omnisorp® 100/360 and Carlo Erba Sorptomatic.
- the analysis Dewar can be raised by a motorized elevator in response to the output of an electronic circuit monitoring the coolant level, as in the Quantachrome Autosorb.
- a porous tube placed around the stem of the sample cell, draws coolant up to the top of that tube by capillary or wicking action, regardless of coolant level around the porous tube, as in several products of Micromeritics.
- the void volume can be reduced further by the use of filler-rods, as taught by U.S. Pat. No. 5,360,743, Lowell. Extreme amounts of said volume filling can be achieved by the use of rods manufactured from polytetra-fluoroethylene (PTFE), as in the Quantachrome® NOVA® analyzer, and can be machined to provide a tighter fit than can rods made of glass.
- PTFE polytetra-fluoroethylene
- the stem portion of the cell can be insulated from the coolant by means of a tight-fitting jacket of material with poor thermal conductivity, or by containment within an evacuated or partially evacuated vessel, which can be silvered as in the manner of a Dewar flask.
- the problems with the prior art control means are that a) through c) require some physical contrivance to actually control the coolant level, which can be less than successful and entails added costs, risk of mechanical and/or electrical failure and normally sets limitations as to the type and size of sample cell and/or Dewar.
- the narrow stems of d) and e) set limitations as to the size of sample which can be admitted into the sample cell.
- tight fitting filler rods can limit evacuation rates of the sample cell; evacuation being a prerequisite for this type of volumetric analysis.
- Insulation means f) is not particularly effective, since it is exactly this type of construction in the surrounding Dewar which is unable to maintain the coolant level, in the first place.
- this prior art adds significant extra cost to the fabrication of the sample cell and increases fragility.
- This invention provides method usable with sorption analyzers for temperature compensation due to coolant level changes around the sample cell. Coolant level changes are due to progressive evaporation of the coolant in the Dewar and cause relative temperature changes in cold and warm zones of the void volume of the analyzer. Such temperature changes generate time-dependent errors in the sorption analysis.
- This invention throughout the duration of a gas sorption analysis, in “real time”, provides temperature compensation, without the need for any physical or mechanical contrivances. Thus, this invention enables correction of the error, otherwise introduced due to the changes in cold and warm zones, in the determination of volumes of gas adsorbed and desorbed.
- This invention permits the coolant to evaporate and, in “real time”, provides for mathematic corrections to the sorption data and the output from the analyzer; a novel solution to the problem.
- the changing coolant level ( ⁇ H) also is employed in a known formula (B) set forth below to obtain the value for the decrease in adsorptive gas in the cold zone ( ⁇ V cold zone) over a given time period.
- the change of that affected portion of the cold zone temperature also is a needed piece(s) of data.
- FIG. 1 is a diagram of the typical sorption analysis system equipment
- FIG. 2 is a flow chart of the operative steps used in the invention
- FIG. 3 is a plot of coolant height vs. time, based upon experimental data
- FIG. 4 is a plot of effected cold zone temperature vs. time, based upon experimental data.
- FIGS. 5 and 5 a show uncorrected and corrected sorption curves, and the amount of correction obtained by this invention.
- the basic system equipment includes: a source 10 of gas, such as nitrogen, under pressure; a source 11 of gas, such as helium, under pressure; a container 12 , termed a Dewar, for coolant 14 , such as liquid nitrogen, fed or prefilled from source 15 ; a sample cell 16 to contain a sample 18 to be analyzed; a valved manifold 19 coupled between the sources 10 and 11 and an input to the sample cell; and various conduits, valves, pressure measuring means, sensors, etc. linking the equipment.
- a computer 20 having the capability of receiving and storing fixed and variable input data; and a readout means 22 , both digital and graphic.
- the analyzer uses only one Dewar 12 , but might have an extra or back up Dewar, and would have a few sample cells 16 , usually of the same and different volumes for extras and for different sample types and volumes.
- the identification of each Dewar 12 and sample cell 16 would be stored in the computer 20 .
- Such identification can include known parameters/data, such as: the volume and internal diameter of the specific Dewar, initial weight of the Dewar when filled with coolant to a specific level, the density of the liquid coolant, external and internal diameter of the stem 21 of the sample cell, the external diameter of any filler rods (not shown in FIG. 1) for the stem, the volume of the manifold 19 , etc.
- the system would have vacuum pump means 23 for evacuating the manifold 19 and the sample cell 16 .
- the sorption system also contains meter means 24 for measuring manifold and sample cell gas pressure at any required time. Based upon stored data and dynamically changing data, the computer 20 can accomplish mathematic tasks, including employing specific polynomials and their coefficients, which can be employed with the present invention.
- the readout means 22 provides the digitized text and plotted information, curves, etc. pertaining to the sorption analysis, as it is being developed over time. A complete analysis, adsorption and desorption can take more than one day, as shown in the plots in FIGS. 3 and 4.
- the computer 20 also contains a program controller portion 25 , which executes one or more established programs, step-by-step. One of the established programs would be the temperature compensation program “TempComp”TM of this invention, one generic embodiment being shown in the flow chart of FIG. 2 .
- the routine tasks for preparing a sample 18 placing it into the sample cell 16 , loading the coolant 14 , such as liquid nitrogen, from the source 15 , into the Dewar 12 , zeroing the system, presetting the system, entering fixed information/data, etc. etc.
- the fixed data would be stored for easy retrieval.
- Variables would be called up by “prompts”, with choices of variables previously stored in the computer memory.
- the first working step could be “#1/select TempComp Sample Analysis”; to call up this unique invention and enable the system to function in a TempComp mode.
- the program could advance through the next several steps.
- the ( ⁇ H) coolant level for a specific Dewar can be stored in the system program/data base by the manufacturer or the user; or it can be determined by equation A as follows, in which W is the weight (mass) of the coolant, the coolant level in the Dewar is (H), (V) is the volume of the Dewar, ( ⁇ ) is the density of the liquid coolant, (D) is the internal diameter of a circular cross-section Dewar and (t i ⁇ t i ⁇ 1 ) is the elapsed time;
- the change of weight ⁇ W is measured “off line” by an accurate scale, over numerous time periods, which can correspond to the BET points, as well as subsequent points in the duration of the sorption analysis.
- this changing coolant level ( ⁇ H) can be loaded in the computer 20 , and recalled/used during analysis, at each specific datum point.
- the storage of such a look up table might not be practical, due to computer memory capacity, etc.
- a conventional curve fitting formula to create a specific equation, which is stored and used via the computer 20 and its program controller 25 .
- One such curve fitting formula (also called a trendline calculating equation) is a least squares fit polynomial:
- ⁇ H (0.1119)+(0.0247)t ⁇ (0.3324 ⁇ 10 ⁇ 6 )t 2 +(0.2933 ⁇ 10 ⁇ 10 )t 3 ⁇ (0.9133 ⁇ 10 ⁇ 15 )t 4 .
- step #2 the program controller would advance to step #2 and determine if all known or fixed data had been input/stored. If not all present, there would be displayed on the screen of the computer 20 and/or readout 22 a request for the missing data, such as the identification of the specific Dewar 12 and the specific sample cell 16 . After manual input of the needed data, the program controller 25 would advance to step #3 and determine if all variable data had been supplied and stored.
- sample cell I.D. which includes the internal diameter of the sample cell (Dcell), and the external diameter of the stem filler rods (Drod) if the rods are used
- Dewar I.D. which includes the internal diameter of the Dewar flask (D) and its volume (V); the density ( ⁇ ) of the liquid coolant; the ( ⁇ H) of the coolant; the weight (W) of the filled Dewar; the initial temperature and rate of temperature change of the cold zone; the number of BET points;
- the computer 20 also would have in memory/storage formulas needed to be used with the fixed and variable data such as the formulas A, B, C, D and the curve fitting polynomials set forth herein, to accomplish the error correction—the “TempComp”.
- Certain of the initial information and the progressively changing data would be transmitted via data lines 26 into the computer, from a sensor array 28 coupled to selected portions of the Dewar, sample cell, gas pressure meter, void volume zones, etc., as is well known in sorption analyzers.
- step #4 the program controller 25 will advance to step #4 and advise the human operator that Analysis can be initialized.
- the system goes through a series of routine sorption analyzer steps: #5 evacuate the sample cell 16 by the pump 23 , via the manifold 19 ; #6 isolate the sample cell by the valve between it and the manifold and build up gas pressure in the manifold 19 from the gas source 11 ; #7 open the valve between the manifold and the sample cell, and wait until pressure equilibrium, measure the new pressure (P) in the manifold and transmit that pressure (P) to computer storage; #8 calculate the void volume (Vcell) of the sample cell from knowing the volume of the gas, such as Helium, which was transferred from the manifold, having a known volume (Vman), into the sample cell, and the change of pressure ( ⁇ P) in the manifold; and store that void volume value.
- the next step #9 causes the sample cell to be immersed in the Dewar which contains the coolant. This is accomplished
- step #10 the pressure change in the cooled sample cell is measured and stored.
- step #11 the warm zone and cold zone volumes are determined.
- the cold zone volume is determined from existing data. Then, it is subtracted from the previously known and stored value of the void volume, to obtain the warm zone volume.
- the changing cold zone volume ( ⁇ V gas cold) is obtained from equation B.
- ⁇ V gas cold ( ⁇ H ⁇ /4) ⁇ (Dcell 2 ⁇ Drod 2 ) ⁇ (P/760);
- step #12 the sample cell is evacuated, the manifold pressure is built up from the adsorptive gas source 10 , to a required amount (Pman), and the valve between the manifold and the sample cell is reopened to enable pressure equilibrium therebetween.
- step #15 the new pressure of the manifold (P′man), which then is the pressure in the sample cell, is measured; and it is used to calculate the total volume of the adsorptive gas transferred into the sample cell by the equation C:
- V TRANS (Pman ⁇ P′man)/760 ⁇ Vman C:
- the volume of the gas thus transferred is recorded and, if this was other than at the first data point of the sorption curve, is added, in step #16, mathematically to the amount(s) previously transferred in step #15 for the previous data point(s), to obtain the current or total ( ⁇ V TRAN ) transferred value.
- the change in stem temperature of the affected is measured as the liquid coolant 14 evaporates from around the upper portion of the stem 21 , progressively during the length of time typical of a full sorption analysis; and that changing temperature data is used to define an experimental temperature in kelvin v. time in minutes the graph 32 , shown in the plot of FIG. 4 .
- T 77.3999+(47336 ⁇ 10 ⁇ 5 )t ⁇ (10819 ⁇ 10 ⁇ 7 )t 2 +(12679 ⁇ 10 ⁇ 1 )t 3 ⁇ (79544 ⁇ 10 ⁇ 14 )t 4 +(25429 ⁇ 10 ⁇ 17 )t 5 ⁇ (33 ⁇ 10 ⁇ 18 )t 5 ,
- step #17 there is determined the temperature corrected volume (V TC ) of the volume of transferred adsorptive ( ⁇ VTRAN) obtained in step #16. Equation D is employed in step #17 as follows:
- V TC ⁇ (r cell 2 ⁇ r rod 2 ) ⁇ ( ⁇ H)+(T/77.4) ⁇ (P/760); D:
- (77.4) is the temperature in kelvin of the liquid coolant
- (P) is the absolute gas pressure in the sample cell in mmHg at that time
- 760 is the standard condition pressure STP.
- V ADS ( ⁇ V TRANS ) ⁇ (V TC +V WARM ZONE +V COLD ZONE ).
- This corrected volume of adsorbate is stored, and recorded by the computer 20 and the readout device 22 , for one of the x-y values of the sorption isotherm shown in solid line 34 in FIG. 5; “x” being the time and “y” being the corrected adsorbate volume.
- steps #13 through #19 are repeated as a loop, with need and use of data for the next isotherm points, to yield x-y output for the next value on the isotherm 34 .
- This process loop of steps #13 to #19 is repeated until all BET and isotherm points are obtained and the sorption analysis is completed. During each cycle through this process loop, many of the data values are different, especially including the coolant height and temperature ( ⁇ H) and (T)corrections.
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Cited By (7)
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US20060027014A1 (en) * | 2004-08-03 | 2006-02-09 | Quantachrome Corporation | Apparatus and method for water sorption measurement |
US20080307905A1 (en) * | 2007-06-15 | 2008-12-18 | Gross Karl J | Thin-Film Sample Holder |
US20090041629A1 (en) * | 2002-05-20 | 2009-02-12 | Gross Karl J | Method and apparatus for measuring gas sorption and desorption properties of materials |
CN103852397A (en) * | 2014-03-11 | 2014-06-11 | 王玉 | Automatic adsorption measuring device by virtue of static volumetric method |
US10222312B2 (en) * | 2016-06-28 | 2019-03-05 | Anton Paar Quantatec, Inc. | Cryogenic temperature controller for volumetric sorption analyzers |
WO2020157646A1 (en) | 2019-01-31 | 2020-08-06 | Anton Paar Quantatec Inc. | Inverted wick type temperature control system for sorption analysis |
US11874155B2 (en) | 2021-04-28 | 2024-01-16 | Micromeritics Instrument Corporation | Systems and methods for gas pycnometer and gas adsorption analyzer calibration |
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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US20090041629A1 (en) * | 2002-05-20 | 2009-02-12 | Gross Karl J | Method and apparatus for measuring gas sorption and desorption properties of materials |
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CN103852397A (en) * | 2014-03-11 | 2014-06-11 | 王玉 | Automatic adsorption measuring device by virtue of static volumetric method |
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WO2020157646A1 (en) | 2019-01-31 | 2020-08-06 | Anton Paar Quantatec Inc. | Inverted wick type temperature control system for sorption analysis |
US10948461B2 (en) * | 2019-01-31 | 2021-03-16 | Anton Paar Quantatec, Inc. | Inverted wick type temperature control system |
DE112020000615T5 (en) | 2019-01-31 | 2021-10-21 | Anton Paar Quantatec Inc. | Inverted wick type temperature control system for sorption analysis |
CN113557422A (en) * | 2019-01-31 | 2021-10-26 | 安东帕量子技术有限公司 | Inverted core type temperature control system for sorption analysis |
US11874155B2 (en) | 2021-04-28 | 2024-01-16 | Micromeritics Instrument Corporation | Systems and methods for gas pycnometer and gas adsorption analyzer calibration |
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